CN110143591A - A kind of compound carbon aerogels of high-specific surface area and preparation method thereof - Google Patents
A kind of compound carbon aerogels of high-specific surface area and preparation method thereof Download PDFInfo
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- CN110143591A CN110143591A CN201910492241.5A CN201910492241A CN110143591A CN 110143591 A CN110143591 A CN 110143591A CN 201910492241 A CN201910492241 A CN 201910492241A CN 110143591 A CN110143591 A CN 110143591A
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- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 57
- 150000001875 compounds Chemical class 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 40
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000000725 suspension Substances 0.000 claims abstract description 27
- 239000002028 Biomass Substances 0.000 claims abstract description 25
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000001913 cellulose Substances 0.000 claims abstract description 8
- 229920002678 cellulose Polymers 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 239000003463 adsorbent Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- 229920001661 Chitosan Polymers 0.000 claims description 8
- 229920002752 Konjac Polymers 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 7
- 239000002041 carbon nanotube Substances 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 6
- 239000002134 carbon nanofiber Substances 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 claims description 5
- 229920002101 Chitin Polymers 0.000 claims description 5
- 229920002581 Glucomannan Polymers 0.000 claims description 5
- 229940046240 glucomannan Drugs 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 2
- 239000012876 carrier material Substances 0.000 claims description 2
- 150000004676 glycans Chemical class 0.000 claims description 2
- 229910001416 lithium ion Inorganic materials 0.000 claims description 2
- 241001312219 Amorphophallus konjac Species 0.000 claims 1
- 235000001206 Amorphophallus rivieri Nutrition 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 12
- 239000001569 carbon dioxide Substances 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 6
- 230000004913 activation Effects 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 abstract 1
- 238000004146 energy storage Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000011232 storage material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 6
- 239000002116 nanohorn Substances 0.000 description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000010583 slow cooling Methods 0.000 description 5
- 235000010413 sodium alginate Nutrition 0.000 description 5
- 239000000661 sodium alginate Substances 0.000 description 5
- 229940005550 sodium alginate Drugs 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 235000010485 konjac Nutrition 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- DGXAGETVRDOQFP-UHFFFAOYSA-N 2,6-dihydroxybenzaldehyde Chemical compound OC1=CC=CC(O)=C1C=O DGXAGETVRDOQFP-UHFFFAOYSA-N 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 125000003147 glycosyl group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- -1 polyethylene Pyrrolidones Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/618—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The present invention relates to compound carbon aerogels of a kind of high-specific surface area and preparation method thereof, the following steps are included: a kind of nano-carbon material is dispersed in water first, a certain amount of PVP dispersing agent is added, disperses in high speed disperser, obtains the suspension of nano-carbon material, biomass material is dispersed in water again, dissolved with vigorous agitation obtains dispersion liquid, and said two devices are mixed, it is vigorously stirred uniformly mixed, obtains nano-carbon material/biology cellulose suspension；- 40 DEG C to -80 DEG C freezing 24-48h, are then freeze-dried, and are then warming up to 700~900 DEG C in an inert atmosphere and keep the temperature 0~6h, obtain compound carbon aerogels.The present invention is not necessarily to exchange of solvent, obtains compound carbon aerogels, specific surface area is up to 3200m after entering carbon dioxide activation2/ g is widely used in the fields such as adsorbent, energy storage material and catalyst and catalyst carrier.
Description
Technical field
The invention belongs to carbon aerogels preparation technical fields, and in particular to a kind of system of the compound carbon aerogels of high-specific surface area
Preparation Method.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
High temperature pyrolysis organic polymer aeroge (such as resorcinol-formaldehyde aeroge) can be prepared under an inert atmosphere
Carbon aerogels, carbon aerogels save aeroge continuously 3-dimensional multi-layered grade cellular structure.But its raw material resorcinol price
High, activity height, easy oxidation by air, therefore need to be protected from light sealing when storage, this just considerably increases the storage cost of raw material.Closely
It is that raw material go to prepare carbon aerogels material, such as cellulose, chitosan, chitin etc., production process that biomass is utilized over year
It is harmless, degradable, inexpensive to human body and ambient enviroment.Biomass-based carbon aerogels are big promising research sides
To.In order to improve the performance and application range of carbon aerogels, nano-carbon material is added among carbon aerogels, can use and receive
The functional group of rice carbon material surface, for example, with cellulose chain strongly mutual can occur for the oxygen-containing functional group on graphene oxide
Effect enhances the performance of composite aerogel and the formation of composite aerogel.
Nano aperture structure on carbon aerogels has the effect that is greatly promoted for improving the performance of material, and then increases
The specific surface area of material, the application of Lai Shixian carbon aerogels more areas.By the nano carbon material with special construction and functionalization
Material is introduced among the three-dimensional porous structure of carbon aerogels, can effectively improve the specific surface areas of carbon aerogels, porosity and
Surface-functional.Since biomass material prepares carbon aerogels material by dissolution-cross-linking process, it is considered to be most simply, most
Convenient, most green preparation method.
Such as: the prior art, which has, prepares carbon nano tube dispersion liquid and the preparation of cellulose crosslinked process using sol-gel method
The method of carbon aerogels material out.But inventor has found: the carbon aerogels material specific surface area of this method preparation is smaller, it is difficult to full
The requirement of the high performance carbon aerogels material of foot.
Summary of the invention
In order to overcome the above problem, the present invention provides a kind of preparation methods of the compound carbon aerogels of high-specific surface area.Benefit
It is mixed with the suspension emulsion of nano-sized carbon with biomass material solution, by the method for In-situ reaction, has prepared high-specific surface area
Compound carbon aerogels, this method carry out in aqueous solution, corrosion-free, green, at low cost, simple process is easily-controllable, raw material sources
Extensively, be conducive to the characteristics of large-scale production.
To realize the above-mentioned technical purpose, The technical solution adopted by the invention is as follows:
A kind of preparation method of the compound carbon aerogels of high-specific surface area, comprising:
Nano-carbon material is uniform with dispersant, and the suspension of nano-carbon material is made of nano-dispersed method；
Biomass material is dispersed in water, biomass material dispersion liquid is formed；
The suspension of nano-carbon material is uniformly mixed with biomass material dispersion liquid, it is fine to form nano-carbon material/biology
Tie up plain suspension；
Above-mentioned nano-carbon material/biology cellulose suspension freezing, freeze-drying, carbonization is compound to get high-specific surface area
Carbon aerogels.
The application research discovery: biomass material is combined with the suspension emulsion of nano-sized carbon, it can be achieved that high-specific surface area
Compound carbon aerogels preparation；Meanwhile specific surface area can be achieved using the combination of the carbon material with Different Pore Structures parameter
Controllable preparation can efficiently control micropore, mesoporous, macropore ratio, and then controllably improve the specific surface of compound carbon aerogels
The structure features such as long-pending and porosity.
Special restriction is not done in the application to the type of nano-carbon material, as long as the nano-carbon material can be introduced into
Among the three-dimensional porous structure of carbon aerogels, and effectively improve the specific surface area, porosity and function of surface of carbon aerogels
Property.Therefore, in some embodiments, the nano-carbon material is graphene oxide, carbon nanotube, carbon nanohorn, carbon are received
Rice any one of fiber or mesoporous carbon.
In order to prepare the suspension of nano-carbon material, the application divides carbon nanomaterial using nano-dispersed machine
It dissipates, but since nano particle is easy to reunite, in order to guarantee dispersion effect, therefore, in some embodiments, the application uses polyethylene
Pyrrolidones PVP is as dispersing agent, the results showed that by the addition of polyvinylpyrrolidone PVP, the dispersed of nanoparticle is obtained
To significantly improving, the suspension good dispersion of the nano-carbon material of preparation.
In some embodiments, the dosage of the application polyvinylpyrrolidone PVP is nano carbon material pulp suspension
5wt% -10wt%.
" nano-dispersed method " refers in the application:, will using various principles, ways and means in liquid medium (such as water)
The aggregate for the various forms that drying nano particle is constituted is reduced into primary particle and it is made to stablize, be uniformly distributed in medium
Technology.In this regard, the application does not make special restriction.In some embodiments, the nano-dispersed method is using nano-dispersed
Machine disperses nano-carbon material and dispersant liquid, to improve dispersion efficiency and convenience.
If jitter time is shorter, the suspension dispersibility of nano-carbon material is poor, easy to reunite, if jitter time is longer, no
Only energy consumption is high and has certain destruction to nano-carbon material itself, therefore, in some embodiments, the high speed disperser pair
The jitter time of nano-carbon material and dispersant liquid is 30-90min.
Biomass refers to the various organisms generated using big gas and water, soil etc. by photosynthesis, i.e., one cuts with life
The organic substance that can be grown of life.Common monosaccharide, polysaccharide and various more complicated natural presomas at present, such as chitin, D-
Grape amine, chitosan, microalgae etc. are used as natural precursor preparation carbon aerogels material, and it is special not do to this in this application
It limits, in some embodiments, the biomass material is chitosan, chitin, sodium alginate, konjaku glucomannan or starch
Any one of.
Research is found: if the dosage of biomass material is too low, the skeleton structure of carbon aerogels is unstable, influences nano carbon material
Effective deposition of material, if the dosage of biomass material is excessively high, nano-carbon material is less, the electric conductivity of carbon aerogels and hole knot
Structure parameter will receive influence, therefore, in some embodiments, the mass ratio of the nano-carbon material and biomass material is 5~
7:2~5.
In some embodiments, the actual conditions of the freezing are to freeze 24-48h at -80~-40 DEG C；
In some embodiments, the actual conditions of carbonization be warming up in an inert atmosphere 700~900 DEG C and keep the temperature 0~
6h。
The present invention also provides the compound carbon aerogels of any above-mentioned method preparation, the compound carbon aerogels specific surfaces
Product >=3200m2/g。
The present invention also provides above-mentioned compound carbon aerogels to prepare catalyst carrier material, adsorbent material, high-performance
Application in supercapacitor or lithium ion battery
The beneficial effects of the present invention are:
(1) it carries out in aqueous solution, it is corrosion-free, green, at low cost, simple process is easily-controllable, raw material sources are wide, is conducive to
The characteristics of large-scale production.
(2) the biomass carbon aerogel material prepared by has graded porous structure, added graphene oxide, and carbon is received
Mitron, carbon nanohorn, the materials such as mesoporous carbon respectively all have unique pore property, with biomass carbon aeroge it is compound after,
Achievable micropore-mesopore is easily adjusted controllably.
The compound of (3) two class carbon materials is not simply to mix, and the suspension emulsion and biomass material solution of nano-sized carbon are mixed
It closes, this is a kind of in-situ compounding process, and it is skeleton that wherein biomass material, which obtains being carbon aerogels, and nano-carbon material conduct
Loaded article is deposited among the skeleton of carbon aerogels.
(4) operating method of the application it is simple, it is at low cost, have universality, be easy to large-scale production.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the konjak portuguese gansu polyose glycosyl carbon aerogels of embodiment 4 and the compound carbon aerogels SEM figure of carbon nano-fiber.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used in this application have logical with the application person of an ordinary skill in the technical field
The identical meanings understood.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
In the examples where no specific technique or condition is specified, according to the literature in the art described technology or conditions or
Person carries out according to product description.Reagents or instruments used without specified manufacturer, being can be by the normal of commercially available acquisition
Advise product.
It is less than normal for the compound carbon aerogels specific surface area prepared at present as background technique is introduced, limit gas
The problem of gelling performance is promoted.Therefore, the present invention proposes a kind of preparation method of carbon aerogels, comprising the following steps:
(1) a kind of nano-carbon material is dispersed in water, a certain amount of PVP dispersing agent is added, in high speed disperser (Germany
IKA, T25 high speed disperser, the range of speeds 3000-25000rpm, peak viscosity 5000mPas) in disperse 30-90min, obtain
To the suspension of nano-carbon material, nano-carbon material includes graphene oxide, carbon nanotube, carbon nanohorn, carbon nano-fiber, Jie
Any one of hole carbon.
(2) a kind of powdered biomass is dissolved in aqueous solution, is vigorously stirred, obtain uniformly mixed solution；Biomass powder
End includes any one of chitosan, chitin, sodium alginate, konjaku glucomannan, starch etc..
(3) (2) two kinds of solution of step (1) and step are mixed, is vigorously stirred using high speed disperser high-speed mixer
To nano-carbon material/biology cellulose suspension, 24-48h is freezed at -80~-40 DEG C, then freeze-drying is mixed
The presoma of carbon aerogels material.
(4) presoma obtained after drying is being warming up to 700~900 DEG C in an inert atmosphere and is keeping the temperature 0~6h, is answered
Close carbon aerogels.
(5) carbon aerogels for obtaining (4) are passed through carbon dioxide gas at 800-1000 DEG C and live in tube furnace
Change, after keeping the temperature 2-4h, then slow cooling, to room temperature, activation obtains the compound carbon aerogels of high-specific surface area.
It is described below by way of scheme of the specific embodiment to the application.In following embodiment, specific surface area is used
Full-automatic specific surface area is tested with lacunarity analysis instrument (U.S. Merck & Co., Inc ASAP2020).
Embodiment 1:
5wt%PVP dispersing agent will be added in 5wt% carbon nano-tube aqueous solutions, at high speed disperser (revolving speed 11000rpm)
The evenly dispersed suspension emulsion of carbon nanotube is obtained after middle dispersion 30min.The sodium alginate of 2wt% is soluble in water, it uses
Sodium alginate soln is obtained after high-speed mixer stirring (5000rpm) 1h, is continued after above two solution is mixed in high-speed stirring
Stirring in machine (5000rpm) is mixed, carbon nanotube/sodium alginate suspension is obtained, freezes 48h at -40 DEG C, be freeze-dried
To the presoma of mixing carbon aerogels.After presoma to be warming up to 900 DEG C in nitrogen and keeps the temperature 4h, it is passed through carbon dioxide gas
(50mL/min) is activated, and after keeping the temperature 2h, then slow cooling is to room temperature, and the compound carbon aerogels after activate, test is tied
Fruit shows: its specific surface area 3200m2/g。
Embodiment 2:
10wt%PVP dispersing agent will be added in 5wt% carbon nanohorn aqueous solution, at high speed disperser (revolving speed 11000rpm)
The evenly dispersed suspension emulsion of carbon nanohorn is obtained after middle dispersion 30min.The chitosan of 2wt% is soluble in water, using height
Chitosan solution is obtained after fast blender stirring (2000rpm) 1h, is continued after above two solution is mixed in high-speed mixer
Stirring, obtains carbon nanohorn/chitosan suspension in (5000rpm), and 48h is freezed at -40 DEG C, and freeze-drying is mixed
The presoma of carbon aerogels.After presoma to be warming up to 900 DEG C in nitrogen and keeps the temperature 4h, it is passed through carbon dioxide gas (40mL/
Min it) is activated, after keeping the temperature 2h, then slow cooling is to room temperature, and the compound carbon aerogels after being activated, test result shows:
Its specific surface area 3150m2/g。
Embodiment 3:
5wt%PVP dispersing agent will be added in 5wt% graphene oxide water solution, in high speed disperser (revolving speed
The evenly dispersed suspension of graphene oxide is obtained after dispersion 30min in 11000rpm).The starch of 2wt% is soluble in water,
Starch solution is obtained after stirring (10000rpm) 1h using high-speed mixer, is continued after above two solution is mixed in high-speed stirring
Stirring in machine (5000rpm) is mixed, graphene oxide/starch suspension is obtained, 48h is freezed at -40 DEG C, freeze-drying obtains
Mix the presoma of carbon aerogels.After presoma to be warming up to 900 DEG C in nitrogen and keeps the temperature 4h, it is passed through carbon dioxide gas
(60mL/min) is activated, and after keeping the temperature 2h, then slow cooling is to room temperature, and the compound carbon aerogels after activate, test is tied
Fruit shows: its specific surface area 3280m2/g。
Embodiment 4:
5wt%PVP dispersing agent will be added in 5wt% carbon nano-fiber aqueous solution, in high speed disperser (revolving speed
The evenly dispersed suspension emulsion of carbon nano-fiber is obtained after dispersion 30min in 11000rpm).By the konjak portuguese gansu polyose of 2wt%
Sugar is soluble in water, konjak portuguese gansu polyose sugar juice is obtained after stirring (5000rpm) 1h using high-speed mixer, by above two solution
Continue the stirring in high-speed mixer (5000rpm) after mixing, obtains carbon nano-fiber/konjaku glucomannan suspension ,-
48h is freezed at 40 DEG C, freeze-drying obtains the presoma of mixing carbon aerogels.Presoma is warming up to 900 DEG C in nitrogen simultaneously
It after keeping the temperature 4h, is passed through carbon dioxide gas (50mL/min) and is activated, after keeping the temperature 2h, then slow cooling is lived to room temperature
Compound carbon aerogels after change, test result show: its specific surface area 3310m2/g。
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to this hair
It is bright, although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still
It can modify to technical solution documented by previous embodiment, or part is equivalently replaced.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to
Make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the compound carbon aerogels of high-specific surface area characterized by comprising
Nano-carbon material is uniform with dispersant, and the suspension of nano-carbon material is made of nano-dispersed method；
Biomass material is dispersed in water, biomass material dispersion liquid is formed；
The suspension of nano-carbon material is uniformly mixed with biomass material dispersion liquid, forms nano-carbon material/biology cellulose
Suspension；
By above-mentioned nano-carbon material/biology cellulose suspension freezing, freeze-drying, it is carbonized to get high-specific surface area composite carbon gas
Gel.
2. the method as described in claim 1, which is characterized in that the nano-carbon material is graphene oxide, carbon nanotube, carbon
Any one of nanometer angle, carbon nano-fiber or mesoporous carbon.
3. the method as described in claim 1, which is characterized in that the dispersing agent is polyvinylpyrrolidone PVP.
4. the method as described in claim 1, which is characterized in that the nano-dispersed method is using high speed disperser to nano-sized carbon
Material is dispersed with dispersant liquid.
5. method as claimed in claim 4, which is characterized in that the high speed disperser is to nano-carbon material and dispersant
The jitter time of liquid is 30-90min.
6. the method as described in claim 1, which is characterized in that the biomass material is chitosan, chitin, Amorphophallus rivieri glucomannan
Any one of glycan, konjaku glucomannan or starch.
7. the method as described in claim 1, which is characterized in that the mass ratio of the nano-carbon material and biomass material is 5
~7:2~5.
8. the method as described in claim 1, which is characterized in that the actual conditions of the freezing are to freeze at -80~-40 DEG C
24-48h；
Or the actual conditions of carbonization are to be warming up to 700~900 DEG C in an inert atmosphere and keep the temperature 0~6h.
9. the compound carbon aerogels of the described in any item method preparations of claim 1-8, which is characterized in that the composite carbon airsetting
Glue specific surface area >=3200m2/g。
10. compound carbon aerogels as claimed in claim 9 are preparing the super electricity of catalyst carrier material, adsorbent material, high-performance
Application in container or lithium ion battery.
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